The effect of support calcination temperature as well as catalyst calcination and reduction temperature on the performance (activity and selectivity) of a Fe:Co/TiO2 catalyst has been investigated. Various techniques (CO chemisorption, TPO, TPR, DSC, BET and Mossbauer Spectroscopy) have been utilized to relate the performance of the above catalyst system to the physical and chemical nature of the catalyst, surface structural stability and various other properties. It was found that a higher support calcination temperature increased the stability of the final catalyst while the catalyst calcination temperature played a lesser role in influencing catalyst performance. Catalyst reduction temperature increased the surface atom ratio, degree of reduction and CO chemisorption, and hence the active metal dispersion, and overall catalytic behaviour.